Earth-treating process and product.



M. J. WELSH.

EARTH TREATING PROCESS AND PRODUCT APPLICATION FILED JAN.26. 1915.

1,1 59,450), Patented Nov. 9, 1915.

INVENTOR J 1 ATI'O R N EY MICHAEL J. WELSH, or PHILADELPHIA, PENNSYLVANIA, .assIGNon To THE ATLANTIC REFIN'ING COMPANY, OF PHILADELPHIA,

PENNsYLvANIA.

PENNSYLVANIA, A COBPOTION OF Specification of Letters Yatent.

Patented Nov. 9, 11915.

Original application filed June 7, 1913, Serial No. 772,415. Divided and this application filed January 26,

- 1915. Serial No. 4,441.

as oils in general, and particularly mineral or petroleum oils, melted paraflin or other wax, stearic acid, etc.

' It is the object of my invention to so treat raw earth, and particularly raw fullers earth, that is, earth which has not been preivously used for decolorizing, purifying, filtering or otherwise acting upon the aforementioned liquids or, any of them, that the earth shall be put into such condition that "it shall retain its useful properties for a longer period; or that a given amount of the material shall be enabled to filter, de. colorize or purify greater quantities of fluid or liquid substance referred to before be-' coming spent or of no further practical value for these purposes or before becoming spent to such degree as to make it necessary or desirable to revivify or reclaim it, as described in my prior application Serial Number 772,415, filed June 7 1913, of which this application is a division and continuation; or that it shall be put in such condition that it shall better withstand or otherwise improve it for further treatment after having been usedupon fluid or liquid substances as described in my.afor.esaid application.

My invention resides in the improved earthymaterial herein described, and in the process of and apparatus for producing the-same. e

, I-shall take the treatment of'fullers earth for illustrative purposes and as the preferred form of my invention.

Floridafullers earth, for 'efiample, is 'first l dried, sothat it'may be granulated and sc'reened to a range of sizes, such, for example, as will-.fpass-through'a 15-mesh screen, notgp'ass through 3118071119811 screen.

This raw granulated earth is then transferred to a roasting or calcining kiln or furnace and heated until it attains a temperature suiiicient to drive off the free moisture, and some of the water of constitution of the fullers earth constituents. While initial drying followed by granulation is the usual and preferred procedure, the earth 'as it'comes from-the mine may be crushed and then treated in any of the ways hereinafter described. After this roasting or calcining treatment the earth is subjected to an aqueous solution of preferably mineral acid, such as sulfuric, nitric or hydrochloric acid, preferably at the boiling temperature.

And while so in contact with the acid. the mass is preferably stirred or agitated. After such acid treatment for a suitable lengthof time, the aqueous solution of'acidand the dissolved earth constituents are drawn off, the remaining liquid being thoroughly washed out, and the remaining .earthy material suitably dried. It may then be used in contactwith any of the liquid substances referred to for filtering, decolorizing, purifying or otherwise acting thereon. 0r, after the earthy material has been washed after acid treatment, it may be driedand again roasted or calcined, and thereafter forthe first time used in contact with any of the liquid. substances referred to. In either case, the acid treatment of the earth causes some of its constituent parts to be dissolved, while other constituents are disintegrated, with the result, however,- that.

the efiiciency of the earth remaining after washing away the acid solutionand the disintegrated constituents is increased. The

more important action, of the acid is that the constituents dissolved or removed are largely the alkaline earths or alkaline earth metals and other constituents which induce, or lend themselves as fluxes in producing, fusion of the earth during the roasting or calcining treatment. The removal of such constituents has the result that in subsequent calcining or roasting treatments there is little orno fusion, and the eficiency of the earth is maintained or improved. By my acid treatment the tzmperature which the'earth will withstand in roasting orcalcining-treatment without producing destructive or undesirable'amount of fusion of the I have found that the acid treatment raises -this incipient fusion point to a good red heat, as distinguished from'a dull red heat for untreated earth. The acid treatment therefore puts the earth in such condition .that it materially resists fusionat the temperature of and at all temperatures lower than that reached in the roasting or calcining treatment. Or the raw earth whether previously dried and granulated ornot, may be subjected to the acid treatment without having been first calcined or roasted as above described. In such case, however, a large proportion of the earth disintegrates and becomes largely nothing but mud. The composition of theraw earth is such that its structure is largely destroyed or disinte-- grated when it is wetted with water or aqueous solution of acid. On the other hand, if the raw earth is first calcined or roasted, the heat causes changes in composi tion, such as driving off of water of constitution, and other changes, and the earth has then sufiicient strength of'structure to admit of treatment by acid solution without losing its desired granular form or porosity.

However, I may, as stated, first treat the ray fullers earth with aqueous solution' of acld, thereby reducing alarge proportion of it to structureless mud, and thereafter washing the mud away. The residue is then calcined or roasted, and such residue comprises material suitable, for-filtering, decolorizing orpurifyingoil or other liquid substance referred-to.

. Besides oils, such as mineral or petroleum oils, other materials in liquid or fluid state "may be operated upon by the earth after the treatment hereinbefore' described or after use upon oil or other liquidorafter the reyivifying or reclaiming treatment described 1n my aforesaid application, and particularly melted paraflin or other wax, or melted stearic acid may be so operated upon? And .w1th respect to the use of the earth upon StBaI'IC acid, it is important that the earth shall have been treated with acid, since earth that has not been treated with acid Wi-ll be attacked as to some of its constituents by the stearic acid, much in the manner of the mineral acid hereinbefore referred to, and the stearic acid by such attack itself becomes more or less neutralized or bonsumed.

In the accompanying drawing I have'illustrated apparatus suitable for the hereinbefore described acid treatment of raw fullers earth or" for the acid treatment of fullers earth which hasbeen used in contact with oily liquid or any of the substances hereinbefore referred to.

In starting a 'treatment of the fullers earth, acid is pumped by acid pump P' trough pipe 1 into the treating tank T. T eacid so-pumped may be weakacid from the weak acid tank A, this, weak acid being v left over from a prior treatment, or strong acid from the strong acid tank A in which case the strong acid is diluted to the proper strength by mlxture with weak. acid or with water, the water being delivered by pump P through pipes 2, 4, 5, 6, 7 and 9. The depth of the acid solution in the tank T is made sufiicient to completely cover the amount of fullrs earth to be treated. The fullers earth, *preferably previously well washed and steamed/if it has been used on oily liquid, is delivered by elevator E into the tank T. As it is being delivered into the mixture is begun and continued until'all the fullers earth of the treatment has been delivered into the acid solution, andthere- 7 after as long as requisite.

Throughout the drawing the various valves are indicated by the reference character '0. It will be understood that these valves may be opened and closedat will, to control delivery ofwthe. materials to the various parts of the apparatus at various times.

The agitation of the mixture above referred to is accomplished by the introduction of air or Water through pipe 4 and flexible hose 5 to the T 6 with which the pipe 7 extending down into the tank T, has a revolu ble air tight 'connestion, a suitable ball-'bearing for the 'pipe and the parts attached thereto being provided at 8. At the lower end of the pipe 7 is attached the pipe 9,

which may be curved, as shown, 1n conformity with the bottom of the tank .T. This pipe 9 has a plurality of lateral perforations, these perforations onone side of the pipe 7.

facing in one'directiqn, and those on the other side of'pipe 7 in another directlon, so

that when water or airunder pressure is de-. livered' through pipe 7 into pipe 9, the water or air escapes through these apertures and the reaction causes the'pipe 9 with its attached pipe 7 to rotate, and during'rotatlon communication is maintained with the "pipe 4 through the T 6. J This rotation of the pipe '9 agitates or mixes the material within the tank T, that is, the acid and fullers earth by carrying around water or air in different parts of the tank T. The T 6 is attached to the chain or cord '11 which passes over the top of the derrick 12 to the windlass 13. By this Windlass the pipe or agitator 9'l'mav beelevated to difierent positions as occasion may require. through the pipes 7 and 9 the valve in In case air'is to be passed I pipe14. leading to the air storage tank A is opened, this tankA being cqnnected by pipe 15 withthe air pump Steam 'admittedtotank T through pipe 3 raises the temperature of the mixture preferably to the boiling'point. 4 Theagitation is kept up for asuitable length of time while the mixture is 'kept near or at the boiling point.- The agitation may then be discontinued for a suitable length of time "and repeated at intervals during the treatment. And throughout the treatment the mixture is kept at or 'near the boiling 7 point as stated. When it is found that the acid ceases or nearly ceases to act, the operation of washing away the 'acid solution or acid solution and disinteand connections situated above the earth line 'in the tank, the liquid in this operation passing off through'the drawofii pipe 16. Prefer ably this, liquid is delivered to the weak acid tank A, any surplus being discharged to the sewer through pipe 1'4. The washing is then continued by filling the tank T with water, mixing it well with the-earth, and allowing the earth to settle, drawing off the water into the sewer through pipes 16 and 17. This washing is continued until the liquid discharged from thetank T is clear and free from acid. When the earth or earthresidue has been satisfactorily washed,

the mass, is agitated while mixed with sufficient water to cause the mixture to readily flow through the bottom cock of tank T into the lower or drying tank or chamber T The water of the mixture is now drained off through the bottom of tank T Steam from the boiler B, super-heated in the super-heater S, is delivered into the tank T now tightly closd at its top, through pipe 19. Thisv steam is forced through the earth from above for the purpose of removing a portion of the waterremaining in the earth and for heating the earth. When the earth has been so treated by steam and thoroughly heated throughout, compressed air, from tank A, heated in. thesuper-heater S, is passed through pipe 20 intothe tank T through the earth. In this. connection it will be understood that the tank T is provided with a perforated false bottom 21 over which is placed a filter cloth of canvas or other suitable material, the steam or air current passing through the earth and out through the false bottom. When 30 B, acid and fifty tons of .earth are used in the abovehours (1 stantially 48 hours for' the washing process before the earth is ready for the drier T thenin condition for treatment of oil or liquid as hereinbefore described. What I claim is:

1. The method of preparing a residue of raw fullers earth or earthy material of similar characteristics for filtering. decolorizing. or purifying liquid, which consists in treat-. ing raw fullers earth or earthy material with acidwvhieh dissolves or extracts ingredients of said earth or earthy material tending to produce fusion, and thereafter wash-. ing the same and separating therefrom the disintegrated structureless portion thereof.

2. The method of preparing a residue of raw fullers earth or earthy material of similar characteristics for percolation of oily liquid therethrough, which consists in treating raw. fullers earth orearthy material with acid which dissolves or extracts ingredients-*of said earth or earthy .material tending to produce fusion, and thereafter washing the same and separating therefrom the I disintegrated structureless .portion thereof.

3. The method of preparing a residue of raw 'fullers earth or earthy material of similar characteristics for filtering, decolor izing or purifying liquid, which consists in treating raw fullers earth or earthy mate rialwith acid which dissolves or extracts ingredients tending to produce fusion, there- 1 structureless portion of said fullersearth or earthy material, and calcining. or roasting the residue.

- 5. The method of preparing raw fullers earth or earthy material of similar characteristics for filtering, decolorizing or purifying liquid, which consists in. calcimngor roasting raw fullers earth: or earthy material, and thereafter treating the same with acid which dissolves or extracts ingredients tending to produce fusion.

6. The method of preparing raw fullers earth or-earthymaterial of slmilar characmentioned treatment, I have found that it requires approximately 96 ation of contact between earth and acid an sub.-..,

teristics for percolation of oily liquid therethrough, which consists in calcining or roasting raw fullers earth or earthy'material, andithereafter treating the same with acid which dissolves or extracts ingredients tending to produce fusion.

7. The method of preparing raw fullers earth for percolationof petroleum oil there= through, which consists in calcining or'roastingraw fullers earth, -and"thereafter treating the same with mineral acid to extract or dissolve ingredients tending to produce fusion. I

8; The-methodof preparing raw fullers earth or earthy material of similar characstructureless portion thereof.

teristics for action upon oily liquid, which consists in calcining or roasting raw fullers earth or earthy 'materiaL-treating the calcined or roasted earth with acid which dissolves or extracts ingredients tending to produce fusion, and thereafter calcining or roasting the earth. I

. 9. The method of preparing raw fullers earth or earthy'material of similar characteristics for action upon oily liquid, which consistsin calcining or roasting raw fullers earth orearthy material, treating thecalcined or roastedearth with acid which dissolves or extracts ingredients tending to produce fusion, and thereafter dryingtheearth: o-

10. A material for filtering, decolorizing or purifying oily liquid consistin of the residue of raw fullers earth remaimngafter extraction therefrom of constituents inducing fusion in calcining or roasting.

extraction therefrom of constituents induc ing fusion in calcining or roasting and after separation therefrom of the disintegrated 12. A material for filtering, decolorizing or purifying oily liquid consisting of the calcined or roasted residue of raw fullers earth remaining after extractlon therefrom of constituents inducing fusion.

13. A material for filtering, decolorizing or purifying liquid consisting of the cal-' cined or roasted residue of raw fullers vearth remaining after extraction therefrom of constituents inducing fusion and separation therefrom of the disintegrated structureless portion thereof.

. In testimony whereof I have hereunto affixed my signature in the presence of the two subscribing witnesses.

MICHAEL JL-WELSH.

Witnesses:

CHARLES E. WAITE, E. B. HENRY. 

